CN101705614A - Preparation method of nickel-plated and silver-plated aromatic polyamide conductive fibers - Google Patents
Preparation method of nickel-plated and silver-plated aromatic polyamide conductive fibers Download PDFInfo
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- CN101705614A CN101705614A CN200910198237A CN200910198237A CN101705614A CN 101705614 A CN101705614 A CN 101705614A CN 200910198237 A CN200910198237 A CN 200910198237A CN 200910198237 A CN200910198237 A CN 200910198237A CN 101705614 A CN101705614 A CN 101705614A
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Abstract
The invention relates to a preparation method of nickel-plated and silver-plated aromatic polyamide conductive fibers, which comprises the following concrete steps of: a. washing and oil removal; b. coarsening: increasing the surface roughness and the surface wettability of fibers; c. sensitizing: soaking the fibers by adopting an aqueous solution formed by stannous chloride and hydrochloric acid; d. activation: soaking the fibers by adopting an aqueous solution formed by palladium chloride and hydrochloric acid; e. chemical nickel plating; f. sensitizing; g. activation; h. chemical silver plating; and i. coating protection. The prepared high performance nickel-plated and silver-plated aromatic polyamide conductive fibers have good electric conductivity, characteristics of heat resistance, flame retardance, light weight and high strength and functions of eliminating static electricity, conducting electricity and transmitting electrical signals. Therefore, the prepared nickel-plated and silver-plated aromatic polyamide conductive fibers can be widely applied to special departments of aviation, space flight, war industry, communication and the like and can also satisfy the clothing and equipment requirements of staffs engaging radars, television relaying and the like.
Description
Technical field
The invention provides a kind of preparation method of high-performance nickel-coated silver-plated aromatic polyamide conductive fibers.
Background technology
Aromatic polyamide fibre (abbreviation aramid fiber) is a kind of high performance organic fiber, mainly (CO-NH-) and the linear high polymer formed of aromatic rings by amido link, have high strength, high-modulus, low-density, heat-proof combustion-resistant, the not fusion of chance naked light, chemical stability waits excellent performance well and is widely used in military project, individual protection field, special industrial circle and composite material reinforcement body or the like.
At aramid fiber surface plating conducting metal, make the fiber surface metallization, can make it have the function of eliminating static, conduction, transmission of electric signals, and have characteristics than metal wire light weight, softness.But aramid fiber surface is smooth, lacks active group, and surface energy is low, reactivity is low, causes chemical plating metal to be difficult to directly in the fiber surface deposition, and fiber and coat of metal adhesion are poor, the coat of metal comes off easily, thereby influences the electric conductivity and the durability of fiber.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high-performance nickel-coated silver-plated aromatic polyamide conductive fibers.
The present invention removes the dirt on the finish of fiber in process and surface by matrix fiber (poly P phenylene diamine terephthalamide fiber or mpd-i fiber or polysulfonamides fibre) is cleaned oil removal treatment earlier; After the oil removing, again fiber surface is carried out roughening and handle, to improve the close attachment fastness of coating and base material; Sensibilization is to adsorb the material that one deck is reduced easily on through the fiber surface after the alligatoring, so that can carry out reduction reaction when activation processing; Activation makes fiber surface form the thin catalytic active layer of one deck; Adopt electroless plating method in the fiber surface plated nickel then; Afterwards, carry out sensitization and activation process again, and then, apply organic protection layer at last, prevent coat of metal oxidation, obtain the high-performance aromatic polyamide conductive fibers in the nickel surface plate silver.
According to above-mentioned mechanism, the present invention adopts following technical scheme:
A kind of preparation method of nickel-plated and silver-plated aromatic polyamide conductive fibers is characterized in that the concrete steps of this method are:
The first step: washing and oil removing, remove fiber surface dirt, finish and impurity;
Second step: alligatoring, the degree of roughness on increased fiber surface and surface wettability;
The 3rd step: sensitization for the first time, the material that absorption one deck is reduced easily on fiber surface;
The 4th step: activation for the first time forms the thin catalytic active layer of one deck at fiber surface;
The 5th step: chemical nickel plating:
A. prepare the nickel plating reactant liquor, wherein each composition and concentration thereof are:
NiSO
420～25g/L, natrium citricum 20～40g/L,
NH
4Cl 30～50g/L, inferior sodium phosphate 15～30g/L;
The pH that regulates above-mentioned nickel plating reactant liquor is 9, will immerse in this reactant liquor through the fiber after washing and oil removing, alligatoring, sensitization for the first time and the activation, and under 45～50 ℃, stirring reaction takes out rinsing after 1～5 minute clean, obtains the fiber that coating surface has nickel;
The 6th step: sensitization for the second time has the material that absorption one deck is reduced easily on the fiber surface of nickel at the 5th step gained coating surface;
The 7th step: activation for the second time forms the thin metal catalytic layer of one deck at the 6th step gained fiber surface;
The 8th step: chemical silvering:
A. prepare silver plating reaction liquid, wherein each composition and concentration are:
AgNO
35～10g/L, ammoniacal liquor 15～50ml/L,
KOH 2～4g/L, glucose or potassium sodium tartrate 10～20g/L,
Ethanol 25～50ml/L, thiocarbamide stabilizing agent 0.2～0.3mg/L;
B. the pH that regulates silver plating reaction liquid is 10～11, to there be the fiber of nickel to immerse in this reactant liquor through the coating surface after the sensitization second time and the activation, under 30～35 ℃, stirring reaction takes out rinsing after 30～60 minutes clean, obtains the conductive fiber that the nickel surface plating has silver.
The 9th step: coating protective prevents the oxidation of the coat of metal.
Above-mentioned aromatic polyamide conductive fibers is poly P phenylene diamine terephthalamide fiber, mpd-i fiber or polysulfonamides fibre.
The washing of the above-mentioned first step and oil removing process are: aromatic polyamide conductive fibers is immersed in the aqueous solution of NaOH and washing agent, wherein concentration sodium hydroxide is: 10g/L～15g/L, and the concentration of washing agent is: 10g/L～25g/L; Under 45 ℃～55 ℃, flood after 10～30 minutes that to take out rinsing clean; Put into acetone soln then, rinsing is taken out in the ultrasonic wave cleaning after 30～60 minutes clean.
The coarsening process in above-mentioned second step is: will put into the coarsening solution alligatoring through the fiber after washing and the oil removing, the preparation method of this coarsening solution is: sodium hydride is put into dimethyl sulfoxide (DMSO), control and add 0.4g～1g sodium hydride in every 100ml dimethyl sulfoxide (DMSO), be heated to 50～60 ℃, reaction does not produce to there being bubble, and filtered while hot obtains coarsening solution.
Above-mentioned first time activation process and for the second time activation process be: will put into by stannous chloride (SnCl through the fiber after washing and oil removing and the alligatoring
2:) and the aqueous solution formed of hydrochloric acid () in, wherein the concentration of stannous chloride is: 10g/L～20g/L, the concentration of hydrochloric acid is: 15ml/L～25ml/L; Under 25～35 ℃, flood after 10～30 minutes that to take out rinsing clean.
Above-mentioned first time of activation and for the second time activation process be: the fiber after the sensitization is put into by palladium bichloride (PdCl
2:) and hydrochloric acid (carry out activation processing in 2～5ml/L) aqueous solution of forming, wherein the concentration of palladium bichloride is: 0.2g/L～0.5g/L, and the concentration of hydrochloric acid is: 2ml/L～5ml/L; Under 25～35 ℃, flood after 10～30 minutes that to take out rinsing clean.
The membrane process that is coated with in above-mentioned the 9th step is: it is in 1～2% the oxine acetum that the fiber after nickel-plated and silver-plated is immersed mass percent concentration, flood taking-up after 2～5 minutes, 45～50 ℃ of vacuum dryings.
The inventive method is by carrying out surface coarsening and etching to aramid fiber, increase the degree of roughness and the surface area of fiber surface, improve the adhesion of the fiber and the coat of metal, pass through fiber surface metal lining electrically conductive layer again, thereby make it have antistatic and conducting function.The high-performance nickel-coated silver-plated aromatic polyamide conductive fibers of the present invention preparation, electric conductivity is good, and has heat-resisting, fire-retardant, light weight, high-strength characteristic, has the function of eliminating static, conduction, transmission of electric signals.Can be widely used in garment industries such as military project, individual protection, special industry.
Description of drawings
Fig. 1 is the picture of aramid fiber after chemical nickel plating is silver-plated of the embodiment of the invention one.
Fig. 2 is the TEM picture of the section of aramid fiber after chemical nickel plating is silver-plated of the embodiment of the invention one.
The specific embodiment
It is matrix fiber that present embodiment adopts the poly P phenylene diamine terephthalamide fiber.
The first step: oil removing, fiber is put into 15g/LNaOH and the 10g/L water-detergent solution soaks, temperature is 50 ℃, takes out after 10 minutes, and is clean with the running water rinsing; Put into acetone soln then, ultrasonic wave cleans after 40 minutes and takes out, and is clean with the running water rinsing.
Second step: alligatoring, fiber is immersed in the 0.1mol/L metallization solvent, room temperature, the taking-up rinsing is clean after 10 minutes.
The 3rd step: sensitization, the aqueous solution of the fiber after the alligatoring being put into 15g/L stannous chloride and 15ml/L hydrochloric acid composition carries out the sensitization processing, and temperature is 30 ℃, takes out rinsing 2～3 times after 20 minutes.
The 4th step: activation, the aqueous solution of the fiber after the alligatoring being put into 0.3g/L palladium bichloride and 3ml/L hydrochloric acid composition carries out the sensitization processing, and temperature is 30 ℃, takes out rinsing 2～3 times after 20 minutes.
The 5th step: a chemical nickel plating, the fiber after the sensitization activation is put into the electroless nickel bath plating.Consisting of of electroless nickel bath: NiSO
4: 20g/L; Natrium citricum: 25g/L; NH
4Cl:38g/L; Inferior sodium phosphate: 18g/L.Sodium hydroxide solution is regulated plating bath pH to 9, and temperature is 48 ℃, and is 2 minutes time, clean with rinsed with deionized water after taking out.
The 6th step: sensitization, with the 3rd step.
The 7th step: activation, with the 4th step.
The 8th step: chemical silvering, the fiber after the nickel plating is put into the silver plating bath plating.Consisting of of chemical plating liquid: AgNO
36g/L; Ammoniacal liquor 20ml/L; KOH 2.5g/L; Glucose 10g/L; Ethanol 30ml/L; Stabilizing agent 0.25mg/L.30 ℃ of temperature, 40 minutes time.
The 9th step: be coated with diaphragm, the fiber behind the chemical silvering put into 1% oxine acetum dipping take out 45～50 ℃ of vacuum dryings after 5 minutes.
Test shows, the resistivity of fiber are 5.8～7.2 μ Ω cm, and the electric conductivity of fiber is good, and has kept the characteristic of original fiber, and is soft, has fire-retardant self-extinguishment.
Claims (7)
1. the preparation method of a nickel-plated and silver-plated aromatic polyamide conductive fibers is characterized in that the concrete steps of this method are:
The first step: washing and oil removing, remove fiber surface dirt, finish and impurity;
Second step: alligatoring, the degree of roughness on increased fiber surface and surface wettability;
The 3rd step: sensitization for the first time, the material that absorption one deck is reduced easily on fiber surface;
The 4th step: activation for the first time forms the thin catalytic active layer of one deck at fiber surface;
The 5th step: chemical nickel plating:
A. prepare the nickel plating reactant liquor, wherein each composition and concentration thereof are:
NiSO
420～25g/L, natrium citricum 20～40g/L,
NH
4Cl 30～50g/L, inferior sodium phosphate 15～30g/L;
The pH that regulates above-mentioned nickel plating reactant liquor is 9, will immerse in this reactant liquor through the fiber after washing and oil removing, alligatoring, sensitization for the first time and the activation, and under 45～50 ℃, stirring reaction takes out rinsing after 1～5 minute clean, obtains the fiber that coating surface has nickel;
The 6th step: sensitization for the second time has the material that absorption one deck is reduced easily on the fiber surface of nickel at the 5th step gained coating surface;
The 7th step: activation for the second time forms the thin metal catalytic layer of one deck at the 6th step gained fiber surface;
The 8th step: chemical silvering:
A. prepare silver plating reaction liquid, wherein each composition and concentration are:
AgNO
35～10g/L, ammoniacal liquor 15～50ml/L,
KOH 2～4g/L, glucose or potassium sodium tartrate 10～20g/L,
Ethanol 25～50ml/L, thiocarbamide stabilizing agent 0.2～0.3mg/L;
B. the pH that regulates silver plating reaction liquid is 10～11, to there be the fiber of nickel to immerse in this reactant liquor through the coating surface after the sensitization second time and the activation, under 30～35 ℃, stirring reaction takes out rinsing after 30～60 minutes clean, obtains the conductive fiber that the nickel surface plating has silver.
The 9th step: coating protective prevents the oxidation of the coat of metal.
2. the preparation method of nickel-plated and silver-plated aromatic polyamide conductive fibers according to claim 1 is characterized in that described aromatic polyamide conductive fibers is poly P phenylene diamine terephthalamide fiber, mpd-i fiber or polysulfonamides fibre.
3. the preparation method of nickel-plated and silver-plated aromatic polyamide conductive fibers according to claim 1, the washing and the oil removing process that it is characterized in that the first step are: aromatic polyamide conductive fibers is immersed in the aqueous solution of NaOH and washing agent, wherein concentration sodium hydroxide is: 10g/L～15g/L, and the concentration of washing agent is: 10g/L～25g/L; Under 45 ℃～55 ℃, flood after 10～30 minutes that to take out rinsing clean; Put into acetone soln then, rinsing is taken out in the ultrasonic wave cleaning after 30～60 minutes clean.
4. the preparation method of nickel-plated and silver-plated aromatic polyamide conductive fibers according to claim 1, the coarsening process that it is characterized in that for second step is: will put into the coarsening solution alligatoring through the fiber after washing and the oil removing, the preparation method of this coarsening solution is: sodium hydride is put into dimethyl sulfoxide (DMSO), control and add 0.4g～1g sodium hydride in every 100ml dimethyl sulfoxide (DMSO), be heated to 50～60 ℃, reaction does not produce to there being bubble, and filtered while hot obtains coarsening solution.
5. the preparation method of nickel-plated and silver-plated aromatic polyamide conductive fibers according to claim 1, it is characterized in that for the first time activation process and for the second time activation process be: will put into by stannous chloride (SnCl through the fiber after washing and oil removing and the alligatoring
2:) and the aqueous solution formed of hydrochloric acid () in, wherein the concentration of stannous chloride is: 10g/L～20g/L, the concentration of hydrochloric acid is: 15ml/L～25ml/L; Under 25～35 ℃, flood after 10～30 minutes that to take out rinsing clean.
6. the preparation method of nickel-plated and silver-plated aromatic polyamide conductive fibers according to claim 1, it is characterized in that activation for the first time and for the second time activation process be: the fiber after the sensitization is put into by palladium bichloride (PdCl
2:) and hydrochloric acid (carry out activation processing in 2～5ml/L) aqueous solution of forming, wherein the concentration of palladium bichloride is: 0.2g/L～0.5g/L, and the concentration of hydrochloric acid is: 2ml/L～5ml/L; Under 25～35 ℃, flood after 10～30 minutes that to take out rinsing clean.
7. the preparation method of nickel-plated and silver-plated aromatic polyamide conductive fibers according to claim 1, the membrane process that is coated with that it is characterized in that for the 9th step is: it is in 1～2% the oxine acetum that the fiber after nickel-plated and silver-plated is immersed mass percent concentration, flood after 2～5 minutes and take out 45～50 ℃ of vacuum dryings.
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| ATE140948T1 (en) * | 1991-03-25 | 1996-08-15 | Du Pont | ELECTROLESS METALIZATION OF ARAMID SURFACES |
| US5302415A (en) * | 1992-12-08 | 1994-04-12 | E. I. Du Pont De Nemours And Company | Electroless plated aramid surfaces and a process for making such surfaces |
| CN1236839A (en) * | 1998-05-21 | 1999-12-01 | 刘绍之 | Electromagnetically shielding fabrics and production method thereof |
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